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Layer-number-controllable graphite film based on nickel-copper composite substrate and preparation method of film

A graphene film and composite substrate technology, applied in the direction of graphene, chemical instruments and methods, coatings, etc., can solve the problems of graphene film size limitation, high hardware investment and preparation cost, complex process, etc., to achieve shape and The effect of less size limitation, strong layer number control ability and wide process window

Active Publication Date: 2012-12-19
SHANGHAI INST OF MICROSYSTEM & INFORMATION TECH CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, thermal evaporation, magnetron sputtering and pulsed laser deposition technology hardware investment and preparation costs are high, and the size of graphene film is limited by large-scale equipment
In addition, patent 201110096201.2 only obtains a single-layer graphene film, while patent 201110266477.0 stated that "by adjusting different reaction temperatures, the spatial distribution range and concentration of carbon also change accordingly, such as the spatial distribution range and concentration of carbon at low temperatures will increase, so as the reaction temperature decreases, the number of graphene layers increases; by controlling the reaction temperature, a graphene film with a continuously adjustable number of layers can be prepared. In the process of controlling the number of layers by the reaction temperature, The interdiffusion between the two metals, the dissolution of carbon on the metal substrate, and the formation of graphene by carbon precipitation are carried out simultaneously, and these dynamic processes are closely related to the temperature of the CVD process. It is necessary to control the number and quality of graphene layers based on experimental experience. quite complicated

Method used

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  • Layer-number-controllable graphite film based on nickel-copper composite substrate and preparation method of film
  • Layer-number-controllable graphite film based on nickel-copper composite substrate and preparation method of film
  • Layer-number-controllable graphite film based on nickel-copper composite substrate and preparation method of film

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] Example 1 Preparation of single-layer graphene

[0040] 1. Experimental method

[0041] 1) Ni-Cu composite substrate: cut copper foil with a thickness of 25μm, the purity of the copper foil is 99.8%, the width is 10cm, and the length is 50cm. The copper foil is cleaned with acetone and isopropanol and dried with nitrogen. Industrial nickel plating process (refer to electrodeposition nanocrystalline material technology for nickel plating method, edited by Tu Zhenmi, etc., National Defense Industry Press, Publication Date: April 1, 2008, ISBN: 9787118055528) was used to form a 150nm metal Ni layer on the Cu surface.

[0042] 2) Carburizing process: use liquid benzene as carbon source, heat to 150-200℃, substrate temperature at 300℃, hold for 30 minutes, Ar flow at 300sccm, H 2 The flow rate is 2sccm.

[0043] 3) Carbon evolution process: cut off the carbon source, raise the substrate temperature to 500°C, keep it for 60 minutes, and the Ar flow rate is 300 sccm, H 2 The flow rat...

Embodiment 2

[0046] Example 2 Preparation of single-layer graphene

[0047] The carbon source is replaced with solid carbon sources such as phenanthrene, pyrene, polystyrene, polymethyl methacrylate, etc. to prepare the graphene film on the nickel-copper composite substrate. Other parameters are the same as in Example 1, and the method is as follows:

[0048] method one:

[0049] 1) Ni-Cu composite substrate: cut copper foil with a thickness of 25μm, the purity of the copper foil is 99.8%, the width is 10cm, and the length is 50cm. The copper foil is cleaned with acetone and isopropanol and dried with nitrogen. Industrial nickel plating process is used to form a 150nm nickel layer on the surface of copper foil.

[0050] 2) Carburizing process: Take phenanthrene as the carbon source, weigh 0.015g of phenanthrene, heat it to 100-150℃, the substrate temperature is 300℃, hold for 60 minutes, and the Ar flow rate is 300sccm.

[0051] 3) Carbon evolution process: Cut off the carbon source, raise the sub...

Embodiment 3

[0068] Example 3 Preparation of multilayer graphene

[0069] 1. Experimental method

[0070] 1) Ni-Cu composite substrate: cut copper foil with a thickness of 25μm, the purity of the copper foil is 99.9%, the width is 20cm, and the length is 20cm. The cut copper foil was cleaned with acetone and isopropanol and then dried with nitrogen. Industrial nickel plating process is used to form a 600nm nickel layer on the surface of copper foil.

[0071] 2) Carburizing process: Using Nai as carbon source, heating to 80~120℃, substrate temperature at 300℃, keeping for 60 minutes, Ar flow at 300sccm, H 2 The flow rate is 2sccm.

[0072] 3) Carbon evolution process: the substrate temperature is increased to 650℃, the temperature is kept for 20-180 minutes, the Ar flow rate is 300sccm, H 2 The flow rate is 1sccm.

[0073] 2. Experimental results: Raman results show that there is carbon signal after 20 minutes of heat preservation, but no graphene, and double layer graphene is formed after 40 minut...

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Abstract

The invention relates to the field of graphite film preparation, and in particular relates to a layer-number-controllable graphite film based on a nickel-copper composite substrate and a preparation method of the film. The preparation method comprises the following steps of: 1) preparing the nickel-copper composite substrate; 2) carburizing, namely heating the nickel-copper composite substrate to 200-300 DEG C, then introducing a carbon source gas and a carrier gas, and carrying out heat preservation for 30-240 minutes for carburization of a nickel layer; and 3) depositing carbon, namely cutting off the supply of the carbon source gas, raising the temperature of the nickel-copper composite substrate to 300-1000 DEG C, introducing the carrier gas, and carrying out heat preservation for 10-180 minutes so as to obtain the graphite film based on the nickel-copper composite substrate. The preparation method has the beneficial effects that a novel preparation process is provided, the layer number of graphite is controlled more easily, the problem that the existing composite substrate is high in preparation cost, and a graphite film material which is low in cost, simple in preparation method, easy to control, good in product quality and large in area is obtained.

Description

Technical field [0001] The invention relates to the field of graphene film preparation, and specifically discloses a graphene film material with a controllable layer number based on a nickel-copper composite substrate and a preparation method thereof. Background technique [0002] Graphene film has important application value because of its good flexibility, mechanical strength and electrical conductivity. Chemical Vapor Deposition (CVD) is the most cost-effective technical way to prepare graphene films. Large-area graphene films can be prepared on metal surfaces such as Cu and Ni, and can be transferred to the surface of various substrates. However, it is difficult to control the number of graphene layers on metal surfaces such as Cu and Ni. The solubility in Ni is large (6.4 to 2.7 at% at 700 to 1000°C). CVD is easy to prepare multilayer graphene, but the number of layers is poor. Due to the low solubility of carbon on the copper surface (<0.001at%, 1000℃), single-layer gra...

Claims

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Application Information

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IPC IPC(8): C30B29/06C23C8/20C23C16/26C01B31/02C01B32/184
Inventor 丁古巧朱云谢晓明江绵恒
Owner SHANGHAI INST OF MICROSYSTEM & INFORMATION TECH CHINESE ACAD OF SCI
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